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EP1914535A1 - Characterisation of gas by optical emission spectrometry - Google Patents

Characterisation of gas by optical emission spectrometry Download PDF

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Publication number
EP1914535A1
EP1914535A1 EP07117940A EP07117940A EP1914535A1 EP 1914535 A1 EP1914535 A1 EP 1914535A1 EP 07117940 A EP07117940 A EP 07117940A EP 07117940 A EP07117940 A EP 07117940A EP 1914535 A1 EP1914535 A1 EP 1914535A1
Authority
EP
European Patent Office
Prior art keywords
pressure
enclosure
valve
gas
analyzer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP07117940A
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German (de)
French (fr)
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EP1914535B1 (en
Inventor
Julien Bounouar
Erwan Godot
Rémi Thollot
Adrien Brouillard
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Alcatel Lucent SAS
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Alcatel Lucent SAS
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Publication of EP1914535A1 publication Critical patent/EP1914535A1/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2226—Sampling from a closed space, e.g. food package, head space
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0011—Sample conditioning
    • G01N33/0016—Sample conditioning by regulating a physical variable, e.g. pressure or temperature
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2226—Sampling from a closed space, e.g. food package, head space
    • G01N2001/2238—Sampling from a closed space, e.g. food package, head space the gas being compressed or pressurized

Definitions

  • the present invention relates to gas characterization by optical emission spectrometry (OES). It relates more particularly to a sampling device for gas analysis.
  • OES optical emission spectrometry
  • Analyzers are known that make it possible today to obtain a qualitative and quantitative measurement of the species present in a gaseous mixture, such as the one whose principle is described in the document US-6643.014 .
  • Such an analyzer comprises a plasma source which excites a mixture of gases present in an enclosure.
  • gaseous species emit photons that are directed to an optical spectrometer emitting via an optical fiber.
  • the Optical Emission Spectrometer separates light into wavelengths. The shape and intensity of the lines of the light intensity spectrum as a function of the wavelengths make it possible to obtain information on the nature of the species present in the gas and their quantity.
  • this analyzer can only be used if the pressure remains constant. If the total pressure is constant, the analyzer makes it possible to follow the evolution of partial pressures of gas. When the total pressure changes, the total intensity of the plasma also changes by modifying the proportions of the partial pressures. Two parameters then vary the proportions of the species simultaneously, which makes any interpretation impossible.
  • the document US.5,986,747 discloses another gas analysis device for performing emission spectrometric measurement on a gaseous mixture present in a main process chamber.
  • the device comprises a small analysis chamber which is connected to the process chamber.
  • the residence time of the gases in the analysis chamber is regulated by a valve and an additional discharge.
  • the additional delivery system can maintain the desired pressure in the analysis chamber regardless of what is happening in the process chamber.
  • the method includes taking a gas sample from the process chamber, isolating the sample in the analysis chamber, exciting the sample in the analysis chamber for radiation, and radiation analysis by a spectrometer.
  • This document relates to the sampling of gas in a process chamber in a pressure range of less than 27 mbar. It does not teach how to characterize gaseous species over a high pressure range up to atmospheric pressure (1 bar) or even beyond,
  • the object of the present invention is to eliminate the drawbacks of the prior art by proposing an analysis system making it possible to associate the variations of intensity of the spectrum only with the variations of partial pressures, and no longer with the variations of power of the the plasma source induced by variations in the total pressure,
  • Another object of the present invention is to enable the analyzer to operate despite a pressure in the chamber that is too high to obtain a plasma, and thus to characterize the gaseous species of a mixture over the entire range of pressures from the pressure.
  • Another aim of the invention is to propose a method and a sampling device for the detection of gaseous species in an enclosure making it possible to maintain a constant pressure at the level of the plasma source, and thus to overcome any variation in pressure in the enclosure.
  • the invention also aims to provide a sampling method and device for the detection of gaseous species in a chamber for continuous measurement in real time.
  • the object of the present invention is a gas sampling device in an enclosure for its analysis communicating on the one hand with an enclosure containing the gas to be analyzed connected to a first pumping group, and on the other hand with a analyzer comprising a chamber containing a gas excitation means and an emission optical spectrometer.
  • the device includes a portion of the pipe connecting the chamber to the analyzer, comprising at least a first pressure-controlled variable conductance valve capable of imposing downstream pressure independent pressure upstream constant flow.
  • the pipe is connected to a second pumping unit to maintain a constant flow in the portion of the pipe included in the device.
  • the downstream pressure P2 acceptable by the analyzer is constant and lower than the upstream pressure P1. It can be seen that the higher the upstream pressure P1, ie the more the pressure in the chamber approaches the atmospheric pressure, the greater the Q / C ratio, therefore the smaller C must be at flow rate Q constant. The conductance C will be smaller the more the valve will be closed.
  • the device comprises at least one variable conductance valve cooperating with an isolation valve.
  • An isolation valve is a valve that can be opened or closed, with upstream and downstream pressures being equal.
  • the pipe portion is formed of at least two parallel branches each comprising a variable conductance valve.
  • variable conductance valve is controlled by a controller so as to maintain a setpoint pressure downstream.
  • the invention also relates to a system for analyzing a gas contained in an enclosure comprising an analyzer, comprising a chamber containing a gas excitation means and a transmission optical spectrometer, and a device as described above.
  • the system communicates with the enclosure via the pumping unit of the enclosure comprising a secondary pump, the device being connected to the discharge of the secondary pump.
  • the sampling device can be placed at the discharge of the secondary pump.
  • the pressure in the pipe is higher than in the enclosure and comprises substantially the same proportions of gaseous species that it is desired to analyze. The pressure difference upstream and downstream of the variable conductance valve is then sufficient to maintain a constant flow and perform a sampling.
  • FIG. 1 represents an enclosure 1 containing the gas to be analyzed connected to a first pumping unit 2 via a pipe 3 provided with a valve 4 .
  • the enclosure 1 may be for example a process chamber, a transfer chamber (load lock), or an entry / exit airlock.
  • the pressure can vary from atmospheric pressure to low pressures of the order of 10 -6 bar.
  • the chamber 1 is also connected to a gas analysis system 5 according to the invention.
  • This system 5 communicates with the enclosure 1 via a pipe 6 connected to a second pumping unit 7 .
  • the system 5 comprises a sampling device 8 .
  • a pressure sensor 9 and an analyzer 10 of reference “APS” of the company “ALCATEL”, comprising an excitation chamber and an optical emission spectrometer (OES), are connected to the duct 6 downstream of the sampling device 8 .
  • the pumping unit 7 advantageously comprises secondary vacuum means so as to obtain a low pressure in the system 5 which provides a clean vacuum, avoiding pollution by the degassing of the walls and the backscattering of the gases of the primary pumping.
  • the reference pump group “DRYTEL” proposed by the company “ALCATEL” meets these criteria since it makes it possible to obtain a molecular vacuum of up to 5.10 -2 mbar for a flow rate of 2.10 -3 mbar.ls -1 at a lower cost and for a small footprint, thanks to a molecular pump known as "molecular drag pump” (MDP).
  • MDP molecular drag pump
  • the channel 6 of the system 5 is chosen with the smallest possible volume in order to avoid the disturbance of the measured by the degassing of the walls or by the dilution of the sample of gas to be measured and in order to obtain a fast response time.
  • the sampling device 8 comprises at least one valve, such as for example an isolation valve 11 and a variable conductance valve 12 controlled by a controller 13. If the variable conductance valve is capable of completely closing the passage it is no longer necessary to add an isolation valve.
  • the variable-conductance valve 12 is disposed on the pipe 6 so that the pressure downstream of the valve 12 is regulated at a chosen set pressure and independent of the pressure upstream of this valve 12. For this purpose, the outlet 14 the signal of the pressure sensor 10 placed downstream of the valve 12 is connected to the controller 13.
  • a plurality of valves with variable conductances can be arranged in parallel so as to better adapt the conductance as a function of the pressure in the chamber 1 , and to cover the entire pressure range comprised between atmospheric pressure and 10 -2 mbar.
  • the portion of the pipe 6 through the sampling device 8 comprises three branches 6a, 6b and 6c arranged in parallel.
  • Each of the ducts 6a, 6b, 6c comprises an isolation valve 11a, 11b and 11c respectively.
  • the lines 6a and 6c each further comprise a variable conductance valve 12a and 12b respectively.
  • a controller 13 manages the openings and closures of the isolation valves 11 and controls the opening / closing of the conductances of the variable conductance valves 12 .
  • the controller 13 may comprise a conventional control system such as a PID corrector (for "Proportional Integral Derivative").
  • the invention aims to maintain a constant pressure acceptable by the analyzer 10 regardless of the pressure inside the enclosure 1 .
  • the sampling is performed at a low flow rate (from 1.10 -2 to 3.10 -1 mbar.ls -1 , and preferably 5.10 -2 mbar.ls -1 ) through a variable-conductance valve 12 pressure-controlled.
  • the pressure downstream of the variable conductance valve 12 is of the order of 50 mbar. From the measurement of the concentration of the gaseous species in the pipe 6 downstream of the variable conductance valve 12 , it is possible to deduce the concentrations of the gaseous species in the chamber 1 .
  • the second pumping group 7 makes it possible to evacuate the gaseous sample flow, but it is necessary, when the chamber 1 is at low pressure, to modify its capacity. pumping to maintain a constant sampling rate. Indeed, at low pressure, the pressure difference upstream and downstream of the variable conductance valve 12 becomes too small to maintain a constant flow rate
  • a restriction 15, such as a variable conductance valve or fixed restriction is placed upstream of the pumping unit 7 to allow to regulate the pumping speed of the pump unit 7 depending on the pressure in the analysis system 5 so as to keep the sampling rate constant,
  • the conductance of the first variable conductance valve 12a is regulated in the closing direction, and the conductance of the second variable conductance valve 12b is regulated in the direction of a plus great opening.
  • variable conductance valve 12 opens to the maximum and the restriction 15 begins to close.
  • the orifice diameter of the conductance of the first variable conductance valve 12a is advantageously less than 1 mm for a gas flow of 1.10 -2 mbar.ls -1 to 50 mbar.ls -1 .
  • the orifice diameter may advantageously be of the order of 2 to 8 mm, and preferably of the order of 5 mm for a flow. from 10 mbar.ls -1 to 2.10 3 mbar.ls -1 .
  • the range of values of the conductance of the second variable conductance valve 12b is wider, and allows flows of 2.10 3 mbar.ls -1 with orifice diameters of the order of 7 mm.
  • valves “132” marketed by the company “CELERITY” are suitable for this purpose. These valves have an extremely short response time, which allows a measurement in real time They take a small gas flow to measure, allowing sampling. And they can regulate pressures of the order of 1 to 100 mbar, which corresponds to the pressure range that is suitable for the "APS" analyzer.
  • FIG. 3 shows another embodiment of the invention in which an enclosure 31 at low pressure is connected to a first pumping unit 32 by a pipe 33 provided with a valve 34.
  • the pumping unit 32 comprises a secondary pump such as a turbomolecular pump.
  • a gas analysis system 35 according to the invention communicates with the enclosure 31 by means of a pipe 36 connected to the discharge of the secondary pump of the pumping unit 32 .
  • the gas analysis system 35 is connected to a second pumping unit 37 .
  • the system 35 comprises a sampling device 38 .
  • a pressure sensor 39 and an analyzer 40 are connected to the pipe 36 downstream of the sampling device 38 .
  • the sampling device 38 according to the invention comprises at least one variable conductance valve disposed on the pipe 36 , such as for example an isolation valve 41 and a variable conductance valve 42 controlled by a controller 43 .

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Food Science & Technology (AREA)
  • Biomedical Technology (AREA)
  • Combustion & Propulsion (AREA)
  • Molecular Biology (AREA)
  • Medicinal Chemistry (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Drying Of Semiconductors (AREA)
  • Control Of Fluid Pressure (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

Le dispositif de prélèvement de gaz dans une enceinte en vue de son analyse communique d'une part avec une enceinte (1) contenant le gaz à analyser, reliée à un premier groupe de pompage (2), et d'autre part avec un analyseur (10) comportant une chambre contenant un moyen d'excitation du gaz et un spectromètre optique à émission. Ce dispositif (8) inclut une portion de la canalisation (6) reliant l'enceinte (1) à l'analyseur (10) comprenant au moins une première vanne (12) à conductance variable contrôlée en pression qui est apte à imposer en aval une pression indépendante de la pression en amont à débit constant. La canalisation (6) est reliée à un deuxième groupe de pompage (7) permettant de maintenir un débit constant dans la portion de la canalisation (6).The gas sampling device in an enclosure for its analysis communicates on the one hand with an enclosure (1) containing the gas to be analyzed, connected to a first pumping group (2), and on the other hand with an analyzer (10) having a chamber containing a gas excitation means and an emission optical spectrometer. This device (8) includes a portion of the pipe (6) connecting the enclosure (1) to the analyzer (10) comprising at least a first pressure-controlled variable conductance valve (12) which is able to impose downstream pressure independent of the upstream pressure at constant flow rate. The pipe (6) is connected to a second pumping unit (7) for maintaining a constant flow in the portion of the pipe (6).

Description

La présente invention se rapporte à la caractérisation de gaz par spectrométrie optique à émission (OES). Elle concerne plus particulièrement un dispositif de prélèvement en vue de l'analyse du gaz.The present invention relates to gas characterization by optical emission spectrometry (OES). It relates more particularly to a sampling device for gas analysis.

L'industrie des semi-conducteurs a un besoin réel de mieux connaître in-situ la composition des mélanges gazeux. On connaît des analyseurs permettant à ce jour d'obtenir une mesure qualitative et quantitative des espèces présentes dans un mélange gazeux, comme celui dont le principe est décrit dans le document US-6,643.014 . Un tel analyseur comporte une source plasma qui excite un mélange de gaz présent dans une enceinte. En se desexcitant, les espèces gazeuses émettent des photons qui sont dirigés vers un spectromètre optique à émission par l'intermédiaire d'une fibre optique. Le spectromètre optique à émission (OES) sépare la lumière en longueurs d'ondes. La forme et intensité des raies du spectre de l'intensité lumineuse en fonction des longueurs d'onde permettent d'obtenir une information sur la nature des espèces présentes dans le gaz et leur quantité.The semiconductor industry has a real need to better know the composition of gaseous mixtures in situ. Analyzers are known that make it possible today to obtain a qualitative and quantitative measurement of the species present in a gaseous mixture, such as the one whose principle is described in the document US-6643.014 . Such an analyzer comprises a plasma source which excites a mixture of gases present in an enclosure. By desexciting, gaseous species emit photons that are directed to an optical spectrometer emitting via an optical fiber. The Optical Emission Spectrometer (OES) separates light into wavelengths. The shape and intensity of the lines of the light intensity spectrum as a function of the wavelengths make it possible to obtain information on the nature of the species present in the gas and their quantity.

Toutefois dans le cadre d'une analyse quantitative des espèces gazeuses, cet analyseur n'est utilisable que si la pression reste constante. Si la pression totale est constante, l'analyseur permet de suivre l'évolution de pressions partielles de gaz. Lorsque la pression totale évolue, l'intensité totale du plasma évolue également en modifiant les proportions des pressions partielles. Deux paramètres font alors varier simultanément les proportions des espèces, ce qui rend toute interprétation impossible.However, in the context of a quantitative analysis of gaseous species, this analyzer can only be used if the pressure remains constant. If the total pressure is constant, the analyzer makes it possible to follow the evolution of partial pressures of gas. When the total pressure changes, the total intensity of the plasma also changes by modifying the proportions of the partial pressures. Two parameters then vary the proportions of the species simultaneously, which makes any interpretation impossible.

Par ailleurs le document US.5,986,747 décrit un autre dispositif d'analyse des gaz permettant de réaliser une mesure par spectrométrie optique à émission sur un mélange gazeux présent dans une chambre de procédé principale. Le dispositif comprend une chambre d'analyse de petite taille qui est reliée à la chambre de procédé. Le temps de résidence des gaz dans la chambre d'analyse est régulé par une vanne et un refoulement supplémentaire. Le système de refoulement supplémentaire peut maintenir la pression désirée dans la chambre d'analyse indépendamment de ce qui se passe dans la chambre de procédé.In addition, the document US.5,986,747 discloses another gas analysis device for performing emission spectrometric measurement on a gaseous mixture present in a main process chamber. The device comprises a small analysis chamber which is connected to the process chamber. The residence time of the gases in the analysis chamber is regulated by a valve and an additional discharge. The additional delivery system can maintain the desired pressure in the analysis chamber regardless of what is happening in the process chamber.

Le procédé comprend le prélèvement d'un échantillon de gaz dans la chambre de procédé, l'isolation de cet échantillon dans la chambre d'analyse, l'excitation de l'échantillon dans la chambre d'analyse pour une radiation, et l'analyse de la radiation par un spectromètre.The method includes taking a gas sample from the process chamber, isolating the sample in the analysis chamber, exciting the sample in the analysis chamber for radiation, and radiation analysis by a spectrometer.

Ce document concerne le prélèvement de gaz dans une chambre de procédé dans une plage de pression inférieure à 27 mbar. Il n'enseigne pas comment caractériser les espèces gazeuses sur une gamme de pression élevée allant jusqu'à la pression atmosphérique (1 bar) ou même au-delà,This document relates to the sampling of gas in a process chamber in a pressure range of less than 27 mbar. It does not teach how to characterize gaseous species over a high pressure range up to atmospheric pressure (1 bar) or even beyond,

La présente invention a pour but d'éliminer les inconvénients de l'art antérieur, en proposant un système d'analyse permettant d'associer les variations d'intensité du spectre seulement aux variations de pressions partielles, et non plus aux variations de puissance de la source plasma induites par des variations de la pression totale,The object of the present invention is to eliminate the drawbacks of the prior art by proposing an analysis system making it possible to associate the variations of intensity of the spectrum only with the variations of partial pressures, and no longer with the variations of power of the the plasma source induced by variations in the total pressure,

La présente invention a aussi comme but de permettre le fonctionnement de l'analyseur malgré une pression dans l'enceinte trop élevée pour obtenir un plasma, et ainsi de caractériser les espèces gazeuses d'un mélange sur toute la gamme de pressions allant de la pression atmosphérique (1 bar) ou de pressions supérieures, à des basses pressions inférieures à 10-2 bar, même si cette pression varie dans le temps.Another object of the present invention is to enable the analyzer to operate despite a pressure in the chamber that is too high to obtain a plasma, and thus to characterize the gaseous species of a mixture over the entire range of pressures from the pressure. atmospheric pressure (1 bar) or higher pressures, at low pressures below 10 -2 bar, even if this pressure varies over time.

L'invention a encore pour but de proposer un procédé et un dispositif de prélèvement en vue de la détection d'espèces gazeuses dans une enceinte permettant de maintenir une pression constante au niveau de la source plasma, et ainsi s'affranchir de toute variation de pression dans l'enceinte.Another aim of the invention is to propose a method and a sampling device for the detection of gaseous species in an enclosure making it possible to maintain a constant pressure at the level of the plasma source, and thus to overcome any variation in pressure in the enclosure.

L'invention a aussi pour but de proposer un procédé et un dispositif de prélèvement en vue de la détection d'espèces gazeuses dans une enceinte permettant une mesure en continu et en temps réel.The invention also aims to provide a sampling method and device for the detection of gaseous species in a chamber for continuous measurement in real time.

L'objet de la présente invention est un dispositif de prélèvement de gaz dans une enceinte en vue de son analyse communiquant d'une part avec une enceinte contenant le gaz à analyser reliée à un premier groupe de pompage, et d'autre part avec un analyseur comportant une chambre contenant un moyen d'excitation du gaz et un spectromètre optique à émission. Le dispositif inclut une portion de la canalisation reliant l'enceinte à l'analyseur, comprenant au moins une première vanne à conductance variable contrôlée en pression apte à imposer en aval une pression indépendante de la pression en amont à débit constant. La canalisation est reliée à un deuxième groupe de pompage permettant de maintenir un débit constant dans la portion de la canalisation incluse dans le dispositif.The object of the present invention is a gas sampling device in an enclosure for its analysis communicating on the one hand with an enclosure containing the gas to be analyzed connected to a first pumping group, and on the other hand with a analyzer comprising a chamber containing a gas excitation means and an emission optical spectrometer. The device includes a portion of the pipe connecting the chamber to the analyzer, comprising at least a first pressure-controlled variable conductance valve capable of imposing downstream pressure independent pressure upstream constant flow. The pipe is connected to a second pumping unit to maintain a constant flow in the portion of the pipe included in the device.

Une vanne à conductance C variable est une vanne qui peut s'ouvrir ou se fermer partiellement de manière à obtenir une pression amont P1 différente de la pression aval P2 à débit Q constant, selon la relation : Q=C(P1-P2). Dans le cas présent, la pression aval P2 acceptable par l'analyseur est constante et inférieure à la pression amont P1. On voit que plus la pression amont P1 est élevée, c'est-à-dire plus la pression dans l'enceinte se rapproche de la pression atmosphérique, plus le rapport Q/C est grand, donc plus C doit être petite à débit Q constant. La conductance C sera d'autant plus petite que la vanne sera plus fermée.A variable conductance valve C is a valve that can partially open or close so as to obtain an upstream pressure P1 different from the downstream pressure P2 at a constant flow rate Q, according to the equation: Q = C (P1-P2). In the case present, the downstream pressure P2 acceptable by the analyzer is constant and lower than the upstream pressure P1. It can be seen that the higher the upstream pressure P1, ie the more the pressure in the chamber approaches the atmospheric pressure, the greater the Q / C ratio, therefore the smaller C must be at flow rate Q constant. The conductance C will be smaller the more the valve will be closed.

Selon une forme d'exécution particulière de l'invention, le dispositif comprend au moins une vanne à conductance variable coopérant avec une vanne d'isolation. Une vanne d'isolation est une vanne qui peut être ouverte ou fermée, les pressions amont et aval étant égales.According to a particular embodiment of the invention, the device comprises at least one variable conductance valve cooperating with an isolation valve. An isolation valve is a valve that can be opened or closed, with upstream and downstream pressures being equal.

Selon un mode de réalisation préféré de l'invention, la portion de canalisation est formée d'au moins deux branches parallèles comprenant chacune une vanne à conductance variable.According to a preferred embodiment of the invention, the pipe portion is formed of at least two parallel branches each comprising a variable conductance valve.

Avantageusement, la vanne à conductance variable est pilotée par un contrôleur de manière à maintenir une pression de consigne en aval.Advantageously, the variable conductance valve is controlled by a controller so as to maintain a setpoint pressure downstream.

L'invention a aussi pour objet un système d'analyse d'un gaz contenu dans une enceinte comprenant un analyseur, comportant une chambre contenant un moyen d'excitation du gaz et un spectromètre optique à émission, et un dispositif tel que décrit précédemment.The invention also relates to a system for analyzing a gas contained in an enclosure comprising an analyzer, comprising a chamber containing a gas excitation means and a transmission optical spectrometer, and a device as described above.

Avantageusement le système communique avec l'enceinte par l'intermédiaire du groupe de pompage de l'enceinte comprenant une pompe secondaire, le dispositif étant connecté au refoulement de la pompe secondaire. De façon alternative, lorsque l'enceinte est maintenue à basse pression au moyen d'un groupe de pompage comportant une pompe secondaire, telle qu'une pompe turbomoléculaire, le dispositif de prélèvement peut être placé au refoulement de la pompe secondaire. Au niveau du refoulement de la pompe secondaire, la pression dans la canalisation est plus élevée que dans l'enceinte et comprend sensiblement les mêmes proportions d'espèces gazeuses que l'on souhaite analyser. La différence de pression en amont et en aval de la vanne à conductance variable est alors suffisante pour conserver un débit constant et réaliser un prélèvement.Advantageously, the system communicates with the enclosure via the pumping unit of the enclosure comprising a secondary pump, the device being connected to the discharge of the secondary pump. Alternatively, when the enclosure is maintained at low pressure by means of a pumping unit comprising a secondary pump, such as a turbomolecular pump, the sampling device can be placed at the discharge of the secondary pump. At the level of the discharge of the secondary pump, the pressure in the pipe is higher than in the enclosure and comprises substantially the same proportions of gaseous species that it is desired to analyze. The pressure difference upstream and downstream of the variable conductance valve is then sufficient to maintain a constant flow and perform a sampling.

D'autres caractéristiques et avantages de la présente invention apparaîtront au cours de la description suivante d'un mode de réalisation, donné bien entendu à titre illustratif et non limitatif, et dans le dessin annexe sur lequel

  • la figure 1 représente une installation comprenant un système d'analyse de gaz selon invention,
  • la figure 2 montre un mode de réalisation du dispositif de prélèvement selon l'invention,
  • la figure 3 montre un autre mode de réalisation du dispositif de prélèvement selon l'invention.
Other characteristics and advantages of the present invention will appear during the following description of an embodiment, given of course by way of illustration and not limitation, and in the accompanying drawing on which
  • FIG. 1 represents an installation comprising a gas analysis system according to the invention,
  • FIG. 2 shows an embodiment of the sampling device according to the invention,
  • Figure 3 shows another embodiment of the sampling device according to the invention.

La figure 1 représente une enceinte 1 contenant le gaz à analyser reliée à un premier groupe de pompage 2 par une canalisation 3 munie d'une vanne 4. L'enceinte 1 peut être par exemple une chambre de procédé, une chambre de transfert (load lock), ou un sas d'entrée / sortie. Dans l'enceinte 1, la pression peut varier depuis la pression atmosphérique jusqu'à des basses pressions de l'ordre de 10-6 bar.FIG. 1 represents an enclosure 1 containing the gas to be analyzed connected to a first pumping unit 2 via a pipe 3 provided with a valve 4 . The enclosure 1 may be for example a process chamber, a transfer chamber (load lock), or an entry / exit airlock. In the chamber 1 , the pressure can vary from atmospheric pressure to low pressures of the order of 10 -6 bar.

L'enceinte 1 est aussi reliée à un système d'analyse de gaz 5 selon l'invention. Ce système 5 communique avec l'enceinte 1 par une canalisation 6 connectée à un second groupe de pompage 7. Le système 5 comprend un dispositif de prélèvement 8. Un capteur de pression 9 et un analyseur 10 de référence «APS» de la société « ALCATEL », comprenant une chambre d'excitation et un spectromètre optique à émission (OES), sont raccordés sur la canalisation 6 en aval du dispositif de prélèvement 8.The chamber 1 is also connected to a gas analysis system 5 according to the invention. This system 5 communicates with the enclosure 1 via a pipe 6 connected to a second pumping unit 7 . The system 5 comprises a sampling device 8 . A pressure sensor 9 and an analyzer 10 of reference "APS" of the company "ALCATEL", comprising an excitation chamber and an optical emission spectrometer (OES), are connected to the duct 6 downstream of the sampling device 8 .

Le groupe de pompage 7 comporte avantageusement des moyens de vide secondaire de manière à obtenir une pression basse dans le système 5 qui procure un vide propre, évitant les pollutions par le dégazage des parois et la rétrodiffusion des gaz du pompage primaire. Le groupe de pompage de référence « DRYTEL » proposé par la société « ALCATEL » répond à ces critères puisqu'il permet d'obtenir un vide moléculaire atteignant 5.10-2 mbar pour un débit de 2.10-3 mbar.l.s-1 à moindre coût et pour un faible encombrement, grâce à une pompe moléculaire dite MDP (de l'anglais « molecular drag pump »), En outre on choisit la canalisation 6 du système 5 avec le volume le plus petit possible afin d'éviter la perturbation de la mesure par le dégazage des parois ou par la dilution de l'échantillon de gaz à mesurer et afin d'obtenir un temps de réponse rapide.The pumping unit 7 advantageously comprises secondary vacuum means so as to obtain a low pressure in the system 5 which provides a clean vacuum, avoiding pollution by the degassing of the walls and the backscattering of the gases of the primary pumping. The reference pump group "DRYTEL" proposed by the company "ALCATEL" meets these criteria since it makes it possible to obtain a molecular vacuum of up to 5.10 -2 mbar for a flow rate of 2.10 -3 mbar.ls -1 at a lower cost and for a small footprint, thanks to a molecular pump known as "molecular drag pump" (MDP). In addition, the channel 6 of the system 5 is chosen with the smallest possible volume in order to avoid the disturbance of the measured by the degassing of the walls or by the dilution of the sample of gas to be measured and in order to obtain a fast response time.

Le dispositif de prélèvement 8 selon l'invention comporte au moins une vanne, comme par exemple une vanne d'isolation 11 et une vanne à conductance variable 12 pilotée par un contrôleur 13. Si la vanne à conductance variable est capable de fermer complètement le passage, il n'est plus nécessaire de lui adjoindre une vanne d'isolation. La vanne 12 à conductance variable est disposée sur la canalisation 6 de telle sorte que la pression en aval de la vanne 12 soit régulée à une pression de consigne choisie et indépendante de la pression en amont de cette vanne 12. A cet effet la sortie 14 du signal du capteur de pression 10 placé en aval de la vanne 12 est reliée au contrôleur 13. The sampling device 8 according to the invention comprises at least one valve, such as for example an isolation valve 11 and a variable conductance valve 12 controlled by a controller 13. If the variable conductance valve is capable of completely closing the passage it is no longer necessary to add an isolation valve. The variable-conductance valve 12 is disposed on the pipe 6 so that the pressure downstream of the valve 12 is regulated at a chosen set pressure and independent of the pressure upstream of this valve 12. For this purpose, the outlet 14 the signal of the pressure sensor 10 placed downstream of the valve 12 is connected to the controller 13.

Selon une forme particulière d'exécution de l'invention, plusieurs vannes à conductances variables peuvent être disposées en parallèle de manière à mieux adapter la conductance en fonction de la pression dans l'enceinte 1, et pour couvrir toute la gamme de pression comprise entre la pression atmosphérique et 10-2 mbar. Dans le mode de réalisation préféré représenté sur la figure 2, la portion de la canalisation 6 traversant le dispositif de prélèvement 8 comprend trois branches 6a, 6b et 6c disposées en parallèle. Chacune des canalisations 6a, 6b, 6c comporte une vanne d'isolation 11a, 11b et 11c respectivement. Les canalisations 6a et 6c comportent chacune en outre une vanne à conductance variable 12a et 12b respectivement.According to a particular embodiment of the invention, a plurality of valves with variable conductances can be arranged in parallel so as to better adapt the conductance as a function of the pressure in the chamber 1 , and to cover the entire pressure range comprised between atmospheric pressure and 10 -2 mbar. In the preferred embodiment shown in Figure 2, the portion of the pipe 6 through the sampling device 8 comprises three branches 6a, 6b and 6c arranged in parallel. Each of the ducts 6a, 6b, 6c comprises an isolation valve 11a, 11b and 11c respectively. The lines 6a and 6c each further comprise a variable conductance valve 12a and 12b respectively.

Un contrôleur 13 gère les ouvertures et fermetures des vannes d'isolation 11 et contrôle l'ouverture/fermeture des conductances des vannes à conductance variable 12. Le contrôleur 13 peut comporter un système de régulation classique tel qu'un correcteur PID (pour « Proportionnel Intégral Dérivé »).A controller 13 manages the openings and closures of the isolation valves 11 and controls the opening / closing of the conductances of the variable conductance valves 12 . The controller 13 may comprise a conventional control system such as a PID corrector (for "Proportional Integral Derivative").

L'invention vise à conserver une pression constante acceptable par l'analyseur 10 quelle que soit la pression à l'intérieur de l'enceinte 1. Pour cela, le prélèvement est effectué à un faible débit (de 1.10-2 à 3.10-1 mbar.l.s-1, et de préférence 5.10-2 mbar.l.s-1) grâce une vanne à conductance variable 12 contrôlée en pression. De cette manière, il est possible de conserver en entrée de l'analyseur 10 une pression suffisamment faible pour permettre d'amorcer le plasma servant à la réalisation de la mesure sur le gaz. Avantageusement la pression en aval de la vanne à conductance variable 12 est de l'ordre de 50 mbar. De la mesure de la concentration des espèces gazeuses dans la canalisation 6 en aval de la vanne à conductance variable 12, on peut déduire les concentrations des espèces gazeuses dans l'enceinte 1.The invention aims to maintain a constant pressure acceptable by the analyzer 10 regardless of the pressure inside the enclosure 1 . For this, the sampling is performed at a low flow rate (from 1.10 -2 to 3.10 -1 mbar.ls -1 , and preferably 5.10 -2 mbar.ls -1 ) through a variable-conductance valve 12 pressure-controlled. In this way, it is possible to keep at the inlet of the analyzer 10 a sufficiently low pressure to allow to initiate the plasma used for carrying out the measurement on the gas. Advantageously, the pressure downstream of the variable conductance valve 12 is of the order of 50 mbar. From the measurement of the concentration of the gaseous species in the pipe 6 downstream of the variable conductance valve 12 , it is possible to deduce the concentrations of the gaseous species in the chamber 1 .

Le second groupe de pompage 7 permet d'évacuer le flux d'échantillon gazeux, mais il est nécessaire, lorsque l'enceinte 1 est à basse pression, de modifier sa capacité de pompage afin de maintenir un débit d'échantillonnage constant. En effet, à basse pression, la différence de pression en amont et en aval de la vanne à conductance variable 12 devient trop faible pour conserver un débit constantThe second pumping group 7 makes it possible to evacuate the gaseous sample flow, but it is necessary, when the chamber 1 is at low pressure, to modify its capacity. pumping to maintain a constant sampling rate. Indeed, at low pressure, the pressure difference upstream and downstream of the variable conductance valve 12 becomes too small to maintain a constant flow rate

Une restriction 15, telle qu'une vanne à conductance variable ou une restriction fixe, est placée en amont du groupe de pompage 7 pour permettre de réguler la vitesse de pompage du groupe de pompage 7 en fonction de la pression dans le système d'analyse 5 de manière à maintenir constant le débit d'échantillonnage,A restriction 15, such as a variable conductance valve or fixed restriction is placed upstream of the pumping unit 7 to allow to regulate the pumping speed of the pump unit 7 depending on the pressure in the analysis system 5 so as to keep the sampling rate constant,

Lorsque la pression dans l'enceinte 1 est élevée, la conductance de la première vanne à conductance variable 12a est régulée dans le sens de la fermeture, et la conductance de la seconde vanne à conductance variable 12b est régulée dans le sens d'une plus grande ouverture.When the pressure in the chamber 1 is high, the conductance of the first variable conductance valve 12a is regulated in the closing direction, and the conductance of the second variable conductance valve 12b is regulated in the direction of a plus great opening.

Lorsque la pression dans l'enceinte diminue, la vanne à conductance variable 12 s'ouvre au maximum et la restriction 15 commence à se fermer.When the pressure in the enclosure decreases, the variable conductance valve 12 opens to the maximum and the restriction 15 begins to close.

Le diamètre d'orifice de la conductance de la première vanne à conductance variable 12a est avantageusement inférieur à 1 mm pour un flux de gaz de 1.10-2 mbar.l.s-1 à 50 mbar.l.s-1. Si une autre vanne à conductance variable 12b est disposée en parallèle de la première vanne 12a, alors le diamètre d'orifice peut avantageusement être de l'ordre de 2 à 8 mm, et de préférence de l'ordre de 5 mm pour un flux de 10 mbar.l.s-1 à 2.103 mbar.l.s-1. La plage de valeurs de la conductance de la seconde vanne à conductance variable 12b est plus étendue, et permet des débits de 2.103 mbar.l.s-1 avec des diamètres d'orifice de l'ordre de 7 mm. Les vannes de référence « 132 » commercialisées par la société « « CELERITY » conviennent à cet usage. Ces vannes possèdent un temps de réponse extrêmement court, ce qui permet de faire une mesure en temps réel Elles prélèvent un petit débit de gaz à mesurer, ce qui permet de réaliser l'échantillonnage. Et elles peuvent réguler des pressions de l'ordre de 1 à 100 mbar, ce qui correspond à la gamme de pression qui convient à l'analyseur « APS ».The orifice diameter of the conductance of the first variable conductance valve 12a is advantageously less than 1 mm for a gas flow of 1.10 -2 mbar.ls -1 to 50 mbar.ls -1 . If another variable conductance valve 12b is disposed in parallel with the first valve 12a , then the orifice diameter may advantageously be of the order of 2 to 8 mm, and preferably of the order of 5 mm for a flow. from 10 mbar.ls -1 to 2.10 3 mbar.ls -1 . The range of values of the conductance of the second variable conductance valve 12b is wider, and allows flows of 2.10 3 mbar.ls -1 with orifice diameters of the order of 7 mm. The reference valves "132" marketed by the company "CELERITY" are suitable for this purpose. These valves have an extremely short response time, which allows a measurement in real time They take a small gas flow to measure, allowing sampling. And they can regulate pressures of the order of 1 to 100 mbar, which corresponds to the pressure range that is suitable for the "APS" analyzer.

La figure 3 représente un autre mode de réalisation de l'invention dans lequel une enceinte 31 à basse pression est reliée à un premier groupe de pompage 32 par une canalisation 33 munie d'une vanne 34. Le groupe de pompage 32 comporte une pompe secondaire telle qu'une pompe turbomoléculaire. Un système d'analyse de gaz 35 selon l'invention communique avec l'enceinte 31 au moyen d'une canalisation 36 connectée au refoulement de la pompe secondaire du groupe de pompage 32.3 shows another embodiment of the invention in which an enclosure 31 at low pressure is connected to a first pumping unit 32 by a pipe 33 provided with a valve 34. The pumping unit 32 comprises a secondary pump such as a turbomolecular pump. A gas analysis system 35 according to the invention communicates with the enclosure 31 by means of a pipe 36 connected to the discharge of the secondary pump of the pumping unit 32 .

Le système d'analyse de gaz 35 est relié à un second groupe de pompage 37. Le système 35 comprend un dispositif de prélèvement 38. Un capteur de pression 39 et un analyseur 40 sont raccordés sur la canalisation 36 en aval du dispositif de prélèvement 38. Le dispositif de prélèvement 38 selon l'invention comporte au moins une vanne à conductance variable disposée sur la canalisation 36, comme par exemple une vanne d'isolation 41 et une vanne à conductance variable 42 pilotée par un contrôleur 43.The gas analysis system 35 is connected to a second pumping unit 37 . The system 35 comprises a sampling device 38 . A pressure sensor 39 and an analyzer 40 are connected to the pipe 36 downstream of the sampling device 38 . The sampling device 38 according to the invention comprises at least one variable conductance valve disposed on the pipe 36 , such as for example an isolation valve 41 and a variable conductance valve 42 controlled by a controller 43 .

Claims (6)

Dispositif de prélèvement de gaz dans une enceinte en vue de son analyse communiquant d'une part avec une enceinte (1) contenant le gaz à analyser, reliée à un premier groupe de pompage (2), et d'autre part avec un analyseur (10) comportant une chambre contenant un moyen d'excitation du gaz et un spectromètre optique à émission, le dispositif (8) incluant une portion de la canalisation (6) reliant l'enceinte (1) à l'analyseur (10), comprenant au moins une première vanne, caractérisé en ce que ladite vanne (12) est à conductance variable contrôlée en pression apte à imposer en aval une pression indépendante de la pression en amont à débit constant, et en ce que ladite canalisation (6) est reliée à un deuxième groupe de pompage (7) permettant de maintenir un débit constant dans la portion de la canalisation (6).Device for sampling gas in an enclosure for analysis communicating on the one hand with an enclosure (1) containing the gas to be analyzed, connected to a first pumping group (2), and on the other hand with an analyzer ( 10) comprising a chamber containing a gas excitation means and an emission optical spectrometer, the device (8) including a portion of the pipe (6) connecting the enclosure (1) to the analyzer (10), comprising at least one first valve, characterized in that said valve (12) is of variable pressure-controlled conductance capable of imposing downstream pressure independent of the upstream pressure at a constant flow rate, and in that said duct (6) is connected a second pumping unit (7) for maintaining a constant flow in the portion of the pipe (6). Dispositif selon la revendication 1, dans lequel la vanne (12) à conductance variable coopère avec une vanne (11) d'isolation.Device according to claim 1, wherein the variable conductance valve (12) cooperates with an isolation valve (11). Dispositif selon l'une des revendications 1 et 2, dans lequel la portion de canalisation (6) est formée d'au moins deux branches (6a, 6c) parallèles comprenant chacune une vanne (12a, 12b) à conductance variable.Device according to one of claims 1 and 2, wherein the channel portion (6) is formed of at least two parallel branches (6a, 6c) each comprising a valve (12a, 12b) of variable conductance. Dispositif selon l'une des revendicatiotis 1 à 3, dans lequel la vanne (12) à conductance variable est pilotée par un contrôleur (13) de manière à maintenir une pression de consigne en aval.Device according to one of claims 1 to 3, wherein the variable conductance valve (12) is controlled by a controller (13) so as to maintain a setpoint pressure downstream. Système d'analyse d'un gaz contenu dans une enceinte comprenant un analyseur, comportant une chambre contenant un moyen d'excitation du gaz et un spectromètre optique à émission, et un dispositif selon l'une des revendications précédentes.System for analyzing a gas contained in an enclosure comprising an analyzer, comprising a chamber containing a gas excitation means and an emission optical spectrometer, and a device according to one of the preceding claims. Système selon la revendication 5, communiquant avec l'enceinte par l'intermédiaire du groupe de pompage de l'enceinte qui comprend une pompe secondaire, le dispositif étant connecté au refoulement de la pompe secondaire.The system of claim 5 communicating with the enclosure via the enclosure pumping unit which includes a secondary pump, the device being connected to the discharge of the secondary pump.
EP07117940A 2006-10-17 2007-10-05 Characterisation of gas by optical emission spectrometry Active EP1914535B1 (en)

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FR0654313A FR2907219B1 (en) 2006-10-17 2006-10-17 GAS CHARACTERIZATION BY OPTICAL EMISSION SPECTROMETRY

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FR3108701B1 (en) * 2020-03-25 2022-02-18 Air Liquide France Ind Gas sampling device

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FR2907219B1 (en) 2008-12-12
FR2907219A1 (en) 2008-04-18
EP1914535B1 (en) 2010-01-20
DE602007004402D1 (en) 2010-03-11

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